EP2064267A2 - Solid polysilane mixtures - Google Patents
Solid polysilane mixturesInfo
- Publication number
- EP2064267A2 EP2064267A2 EP07817520A EP07817520A EP2064267A2 EP 2064267 A2 EP2064267 A2 EP 2064267A2 EP 07817520 A EP07817520 A EP 07817520A EP 07817520 A EP07817520 A EP 07817520A EP 2064267 A2 EP2064267 A2 EP 2064267A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- mixtures
- polysilanes
- solid
- polysilane
- polysilanes according
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/60—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
Definitions
- the invention relates to solid mixtures of polysilanes whose individual components decompose and which are obtained from the hydrogenation of plasma-chemically generated largely halogenated, preferably fluorinated, particularly preferably chlorinated Polysilanmischungen.
- polysilanes are generally compounds of the composition Si n H 2n or Si n H 2n + 2 where n> 1.
- Polysilanes may contain linear si n chains and / or Si n rings, as well as chain branches. exhibit.
- Polysilanes of the composition Si n H 2n or Si n H 2n + 2 are denoted by n> 10, preferably n> 12, as high molecular weight polysilanes or high molecular weight polysilanes according to the invention, this corresponds to molar masses of more than 350 g / mol.
- polysilanes are referred to, which are solid at room temperature, as solid mixtures of polysilanes mixtures of polysilanes whose individual components are solid at room temperature.
- boiling is defined as a state in which the vapor pressure of a substance corresponds to the applied process pressure, the boiling point in the sense of the invention being the temperature at which the vapor pressure of a substance reaches the applied process pressure.
- the substance may be in the liquid or solid state at the boiling point and during boiling. This explicitly includes sublimation, the direct transition from solids to the gas state. If the decomposition temperature of a substance is reached before it begins to boil, then the boiling point of the substance under the applied process pressure is the temperature at which, based on the vapor pressure curve of the substance, it would theoretically boil.
- Hydrogen-substituted polysilanes with high boiling points are suitable for the production of Silici ⁇ m-Schlvier or Sillcl ⁇ m structures, since solutions of the Polysilanes in solvents with a lower boiling point than that of the dissolved polysilanes selectively applied, the solvent removed and the remaining high-boiling polysilanes can be decomposed by suitable processing to silicon (Nature 2006, 440, 783-786).
- EP 1087428 A1 describes that solutions of polysilanes can be applied in a targeted manner by means of ink-jet processes in order to arrive at silicon structures.
- EP 1085579 A1 discloses that, by suitable methods, such solutions can be applied over a wide area in order to produce thin films of silicon.
- EP 1357154 A1 discloses that a particular advantage of using high molecular weight polysilanes compared to polysilanes with low boiling points is the possibility of process control close to atmospheric pressure and the avoidance of CVD method. At the same time, high molecular weight polysilanes are safer to handle than low molecular weight because they are less prone to auto-ignition due to their lower vapor pressure and lower reactivity with air.
- a disadvantage of the process described in EP 1357154 A1 for the preparation of the polysilane mixtures used in the prior art is the complex, multistage process in which first low molecular weight polysilanes are synthesized which are then partially subjected to photochemical chain extension in order to obtain a usable polysilane mixture with high-boiling fractions reach.
- low-boiling polysiams are lost through evaporation or must be separated from the high-boiling fractions by suitable separation techniques prior to processing the polysilane mixture.
- the rapid decomposition of polysilanes to silicon begins at about 300 ° C.
- the polysilanes used should be under the used process pressure do not boil below the decomposition temperature.
- the boiling point of a polysilane at a given pressure increases with increasing molecular weight. It is known that, for chain-type polysilanes and atmospheric pressure, a boiling point of about 300 ° C. is achieved with the decasilane Si 10 H 22 , a boiling point of about 350 ° C. with the tridekasiane Si 13 H 28 .
- the melting points of the corresponding polysilanes are above 0 ° C, already the dodecasifan Si 12 H 26 is solid at room temperature. Accordingly, mixtures of polysilanes, the components of which are solid at room temperature, are particularly suitable for allowing decomposition to silicon with low evaporation rates.
- DE 102005024041.0 discloses that mixtures of largely chlorinated polysilanes can be obtained by reaction of SiCl 4 with H 2 in a plasma process at low temperature.
- the object of the invention is to provide polysilane mixtures with high boiling points and sufficient solubility, the synthesis of which is simplified in comparison to the prior art and thus less expensive.
- the object is achieved by hydrogenating a mixture of substantially chlorinated polysilanes, produced according to DE 102005024041.0, without further purification in suitable processes, and then obtaining solid mixtures of polysides by suitable aftertreatment.
- the object is achieved by hydrogenating this fraction in suitable processes according to a fractionation with separation of the desired high molecular weight fraction of the chloropolysilane mixtures as described in DE 102006 034061.2 and appropriately treating the resultant mixture of hydrogenated polysilanes to obtain a solid mixture of polysilanes ,
- the polysilanes volatile below their decomposition temperature below the desired process pressure can be separated, for example, by atmospheric pressure distillation or distillation under reduced pressure. These volatile polysilanes can be further used for the precipitation of silicon layers in gas phase processes, for example CVD processes.
- the separation of the polysilanes of insufficient molecular weight may be effected by suitable solvents or solvent mixtures in which polysilanes of suitable molecular mass, in contrast to those of lower molecular mass, are less or more soluble.
- a separation of the resulting solutions from the solid Röckpartyn can be done for example by filtration or centrifugation.
- the separation of the polysilanes of insufficient molecular weight can be carried out by chromatographic methods, for example GPC or HPLC.
- a solvent for solid polysilane mixtures can serve low molecular weight polysilanes, which are removed after application of the liquid by suitable methods on a substrate by evaporation.
- Liquids are used which do not react with components of the Poiysilanmischungen under the handling conditions and have a boiling point which is below the decomposition temperature of the Polysilanmischungen.
- Solid polysilane mixtures can be applied as solids to surfaces and, after application by heat treatment, melted to produce liquid polysilicon structures or polysilane films which are thereafter decomposed to silicon by suitable methods.
- Solid polysilane mixtures can form dispersions with solvents or solvent mixtures in which the polysilanes are only partially dissolved. Sufficiently small sizes of the dispersed polysilane particles further permit processing into homogeneous polysilicon structures or polysilane layers, especially if the process temperatures result in melting of the remaining polysilane mixture after evaporation of the solvent or solvent mixture.
- the compounds or dispersions of the solid polysilane mixtures may be admixed with further compounds in a suitable amount which comprise, for example, at least one element of the main groups I or V of the Periodic Table of the Elements,
- the compounds admixed to the solid polysilane mixtures or their solutions or dispersions preferably have boiling points below the applied process pressure which are at least as high as the decomposition temperatures of the polysilane mixtures, more preferably decompose at temperatures similar to those of the polysilane mixtures, so that the concentrations of the admixed elements in the resulting silicon can be controlled and predicted.
- Solid polysilane mixtures oxidize slowly under air contact, but are not self-igniting. The solid ignited in air with a flame goes out automatically when removing the ignition source and in the absence of an additional heat source.
- solid polysilane mixtures before further use of the solid polysilane mixtures, it proves to be advantageous to store them in a transport container whose surface is made light-tight and the interior of which is acted upon by the inert Polysilangemisch with an inert gas. It also proves to be advantageous to provide this transport container with a take-off device with which the solid Polysilangemisch dosed withdrawn and can be supplied for further use.
- the mixtures can be processed into shaped articles, for example pellets or rods.
- the production of moldings may be associated with the addition of additives in order to promote the cohesion of the moldings and / or to reduce the Oxidungsempfind ⁇ ndige of the polysilanes contained.
- the production of the moldings can take place up to temperatures at which the polysilane mixtures solid at room temperature melt completely or partially, but do not yet decompose.
- the shaped bodies can also be subsequently coated with a functional layer which, for example, reduces abrasion, improves the cohesion of the shaped bodies and / or reduces the oxidation sensitivity of the shaped bodies.
- the substances used as aggregates or coating materials should not be mixed with the components of the processing temperatures
- Polysilane mixtures react and either selectively before or during the preparation of Polysilanariaen or dispersions of the polysilanes or, if they remain in the solution or dispersion of Polysilanmischungen, under the applied process pressure from the surface evaporate on which silicon is to be produced before the decomposition temperature of the Potysilanmischungen is reached in order to avoid contamination of the resulting Silicium Modellen or layers.
- Polysilane mixture are dissolved in 350 ml_ benzene and added dropwise with stirring at 0 ° C 180 mL of a 1 M LiAIH 4 solution in diethyl ether. Thereafter, allow to warm slowly to room temperature. After a total of 24 h, the solid precipitate is filtered off and washed with benzene. The residue is extracted to remove lithium salts with a total of 400 mL of absolute ethanol at room temperature and the residue is isolated 3.85 g of solid Polysifanmischung.
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
- Silicon Compounds (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102006043929.5A DE102006043929B4 (en) | 2006-09-14 | 2006-09-14 | Process for the preparation of solid polysilane mixtures |
PCT/DE2007/001648 WO2008031427A2 (en) | 2006-09-14 | 2007-09-13 | Solid polysilane mixtures |
Publications (1)
Publication Number | Publication Date |
---|---|
EP2064267A2 true EP2064267A2 (en) | 2009-06-03 |
Family
ID=39104926
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP07817520A Withdrawn EP2064267A2 (en) | 2006-09-14 | 2007-09-13 | Solid polysilane mixtures |
Country Status (4)
Country | Link |
---|---|
US (1) | US8177943B2 (en) |
EP (1) | EP2064267A2 (en) |
DE (1) | DE102006043929B4 (en) |
WO (1) | WO2008031427A2 (en) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102008025261B4 (en) | 2008-05-27 | 2010-03-18 | Rev Renewable Energy Ventures, Inc. | Halogenated polysilane and plasma-chemical process for its preparation |
DE102008025260B4 (en) | 2008-05-27 | 2010-03-18 | Rev Renewable Energy Ventures, Inc. | Halogenated polysilane and thermal process for its preparation |
DE102010025710A1 (en) | 2010-06-30 | 2012-01-05 | Spawnt Private S.À.R.L. | Storage material and process for recovering H-silanes therefrom |
DE102010025948A1 (en) | 2010-07-02 | 2012-01-05 | Spawnt Private S.À.R.L. | Medium chain polysilanes and process for their preparation |
DE102010032075A1 (en) | 2010-07-23 | 2012-01-26 | Eads Deutschland Gmbh | Hydrogen production by means of hydrogenated polysilanes for the operation of fuel cells |
DE102013207444A1 (en) * | 2013-04-24 | 2014-10-30 | Evonik Degussa Gmbh | Process and apparatus for the production of polychlorosilanes |
DE102013207447A1 (en) * | 2013-04-24 | 2014-10-30 | Evonik Degussa Gmbh | Process and apparatus for the preparation of octachlorotrisilane |
WO2016095953A1 (en) * | 2014-12-15 | 2016-06-23 | Spawnt Private S.À.R.L. | Method for producing chlorinated oligosilanes |
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-
2006
- 2006-09-14 DE DE102006043929.5A patent/DE102006043929B4/en not_active Expired - Fee Related
-
2007
- 2007-09-13 EP EP07817520A patent/EP2064267A2/en not_active Withdrawn
- 2007-09-13 WO PCT/DE2007/001648 patent/WO2008031427A2/en active Application Filing
-
2009
- 2009-03-12 US US12/402,852 patent/US8177943B2/en not_active Expired - Fee Related
Non-Patent Citations (2)
Title |
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None * |
See also references of WO2008031427A2 * |
Also Published As
Publication number | Publication date |
---|---|
WO2008031427A3 (en) | 2008-12-11 |
WO2008031427A2 (en) | 2008-03-20 |
DE102006043929A1 (en) | 2008-03-27 |
US8177943B2 (en) | 2012-05-15 |
US20100004385A1 (en) | 2010-01-07 |
DE102006043929B4 (en) | 2016-10-06 |
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Inventor name: BAUCH, CHRISTIAN Inventor name: AUNER, NORBERT Inventor name: DELTSCHEW, RUMEN Inventor name: MOHSSENI-ALA, SEYED-JAVAD Inventor name: LIPPOLD, GERD Inventor name: HOLL, SVEN |
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Inventor name: LIPPOLD, GERD Inventor name: AUNER, NORBERT Inventor name: MOHSSENI-ALA, SEYED-JAVAD Inventor name: BAUCH, CHRISTIAN Inventor name: DELTSCHEW, RUMEN Inventor name: HOLL, SVEN |
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